HRID510395

反应详情

EQUATION

反应方程式

HRID 510395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of ethyl 3-(2-chlorophenyl)-2-cyanopropanoate (2.37 g, 10 mmol) in ethanol (20 mL) and acetic acid (20 mL) under nitrogen was added hydrazine monohydrate (2.5 g, 49.9 mmol). The reaction mixture was heated and stirred at 100° C. overnight. Reaction mixture was concentrated. Oily residue was dissolved with ethyl acetate (60 mL) and 5% HCl solution (15 mL). Two layers were separated. Organic layer was washed with brine (15 mL), dried and concentrated to give product. It was used in next step without purification. (1.98 g, 89%); LC/MS: MS (ES+) m/e 224 (MH+)

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. customReaction mixture
  3. concentrationwas concentrated
  4. dissolutionOily residue was dissolved with ethyl acetate (60 mL) and 5% HCl solution (15 mL)
  5. customTwo layers were separated
  6. washOrganic layer was washed with brine (15 mL)
  7. customdried
  8. concentrationconcentrated
  9. customto give product
  10. customIt was used in next step without purification